化工社化工社 化学情報印刷レポート · 研究参考用
Potassium Hydroxide → 2-Methyl-3,4,6-trifluorobenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Pentaethylenehexamine | HCID 19990 | — |
| 反応物 | 2,3,4,5-Tetrafluoro-6-methylbenzoic acid | HCID 12943997 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Palladium hydroxide | HCID 9942167 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Methyl-3,4,6-trifluorobenzoic acid | HCID 10130305 | 80.1% |
反応手順
To a solution of 1.04 g of 2,3,4,5-tetrafluoro-6-methylbenzoic acid in 15 ml of ethanol were added 840 mg of potassium hydroxide, 232 mg of pentaethylene hexamine and 200 mg of 20% palladium hydroxide. The mixture was stirred in a hydrogen atmosphere at room temperature for 3 hours. After addition of water, the reaction mixture was filtrated through celite and the filtrate was washed with diethyl ether. The aqueous layer was adjusted to pH 1 with concentrated hydrochloric acid and extracted with dichloromethane. After evaporating the solvent, the residue was purified by silica gel column chromatography (eluent; ethyl acetate:n-hexane=1:3) to give 761 mg of 3,4,6-trifluoro-2-methylbenzoic acid (yield: 80%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06333431B1 |
| 出典データセット | uspto-grants-2001_12 |
| ORD ID | ord-a963873675e54885aaadf31bcd845358 |
| 出典メモ | uspto-grants-2001_12 |